反応 #49175

ord-d8e7cc59633842469a6293c295a59251

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他evaporated dryness
  2. 2
    workup.DISSOLUTIONThe residue was dissolved in dichloromethane (300 mL)
  3. 3
    洗浄It was washed with saturated NaHCO3 aqueous solution (3×100 mL)
  4. 4
    乾燥The organic layer was dried over Na2SO4
  5. 5
    ろ過filtered
  6. 6
    その他evaporated to dryness

実験手順

Compound 17 (10.5 g, 22 mmol) was dissolved in anhydrous dichloromethane (150 mL). To the solution were added disuccinimidyl carbonate (8.45 g, 33 mmol), triethylamine (20 mL) and acetonitrile (50 mL). The reaction mixture was stirred at room temperature under argon for over night and then evaporated dryness. The residue was dissolved in dichloromethane (300 mL). It was washed with saturated NaHCO3 aqueous solution (3×100 mL). The organic layer was dried over Na2SO4, filtered and evaporated to dryness. Compound 18 (10.4 g, 77%) was obtained as colorless powder after drying in high vacuum, which was directly used for the next step without further purification.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07745608B2uspto-grants-2010_06